# Electronic Supplementary Material (ESI) for CrystEngComm.
# This journal is © The Royal Society of Chemistry 2022

####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
#######################################################################

data_Independent_Atom_Model
_database_code_depnum_ccdc_archive 'CCDC 2181471'
loop_
_audit_author_name
_audit_author_address
'Roman Gajda'
;University of Warsaw
Poland
;
_audit_update_record             
;
2022-06-23 deposited with the CCDC.	2022-09-07 downloaded from the CCDC.
;
_audit_creation_date             2022-06-23
_audit_creation_method           
;
Olex2 1.5
(compiled 2022.04.07 svn.rca3783a0 for OlexSys, GUI svn.r6498)
;
_shelx_SHELXL_version_number     2018/3
_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         'B4 H4 O9, 2(H4 N), 2(H2 O)'
_chemical_formula_sum            'B4 H16 N2 O11'
_chemical_formula_weight         263.39
_chemical_absolute_configuration ?
_chemical_melting_point          ?
_chemical_oxdiff_formula         B4O11N2H16
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
B B 0.0013 0.0007 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_shelx_space_group_comment       
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;
_space_group_crystal_system      monoclinic
_space_group_IT_number           4
_space_group_name_H-M_alt        'P 1 21 1'
_space_group_name_Hall           'P 2yb'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, y+1/2, -z'

_cell_length_a                   7.16499(7)
_cell_length_b                   10.59066(11)
_cell_length_c                   7.24742(6)
_cell_angle_alpha                90
_cell_angle_beta                 98.6290(9)
_cell_angle_gamma                90
_cell_volume                     543.723(9)
_cell_formula_units_Z            2
_cell_measurement_reflns_used    51795
_cell_measurement_temperature    90.1(6)
_cell_measurement_theta_max      65.9010
_cell_measurement_theta_min      3.4460
_shelx_estimated_absorpt_T_max   ?
_shelx_estimated_absorpt_T_min   ?
_exptl_absorpt_coefficient_mu    0.159
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.73842
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.42.36a (Rigaku Oxford Diffraction, 2021)
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.609
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       irregular
_exptl_crystal_F_000             276
_exptl_crystal_size_max          0.27
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.12
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0555
_diffrn_reflns_av_unetI/netI     0.0410
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.997
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       26
_diffrn_reflns_limit_k_min       -26
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            94540
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.992
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         62.671
_diffrn_reflns_theta_min         3.433
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      90.1(6)
_diffrn_detector                 'Hybrid Pixel Array Detector'
_diffrn_detector_area_resol_mean 10.0000
_diffrn_detector_type            HyPix
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_details      
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  tₑₓₚ   ω     θ     κ     φ   Frames
#--------------------------------------------------------------------------
  1  ω    -74.00  10.00   0.50   20.00    --  -33.40  72.00-155.00  168
  2  ω    -74.00 -48.00   0.50   20.00    --  -33.40 -72.00  74.00   52
  3  ω     -3.00 116.00   0.50   20.00    --   33.40  72.00-155.00  238
  4  ω    -13.00  40.00   0.50   20.00    --   33.40 -72.00  74.00  106
  5  ω    -72.00 -47.00   0.50   62.00    --  -92.00  72.00-155.00   50
  6  ω   -144.00 -51.00   0.50   62.00    --  -92.00 -72.00  74.00  186
  7  ω     58.00 157.00   0.50   62.00    --   99.01  72.00-155.00  198
  8  ω     43.00  79.00   0.50   62.00    --   99.01 -72.00  74.00   72
  9  ω     43.00  96.00   0.50   20.00    --   33.40 178.00  60.00  106
 10  ω     42.00 122.00   0.50   20.00    --   33.40 178.00 -30.00  160
 11  ω      1.00 113.00   0.50   20.00    --   33.40  57.00-180.00  224
 12  ω     32.00 119.00   0.50   20.00    --   33.40  77.00 -90.00  174
 13  ω     29.00  55.00   0.50   20.00    --   33.40  77.00   0.00   52
 14  ω     45.00 112.00   0.50   20.00    --   33.40 178.00  90.00  134
 15  ω     42.00 116.00   0.50   20.00    --   33.40 178.00-180.00  148
 16  ω     -8.00  18.00   0.50   20.00    --   33.40  77.00   0.00   52
 17  ω      0.00 108.00   0.50   20.00    --   33.40  57.00  60.00  216
 18  ω      0.00  26.00   0.50   20.00    --   33.40  77.00 -90.00   52
 19  ω     -2.00 113.00   0.50   20.00    --   33.40  57.00 -30.00  230
 20  ω     -9.00 112.00   0.50   20.00    --   33.40  77.00  90.00  242
 21  ω     70.00  98.00   0.50   20.00    --   33.40  77.00   0.00   56
 22  ω   -162.00-136.00   0.50   62.00    --  -92.00 -76.00  94.53   52
 23  ω    -74.00 -49.00   0.50   62.00    --  -92.00 -76.00-162.48   50
 24  ω   -172.00-111.00   0.50   62.00    --  -92.00 -77.00 -57.99  122
 25  ω   -131.00-105.00   0.50   62.00    --  -92.00 -76.00-162.48   52
 26  ω    -74.00 -49.00   0.50   62.00    --  -92.00 -77.00-180.00   50
 27  ω    -74.00 -49.00   0.50   62.00    --  -92.00 -77.00 -57.99   50
 28  ω    -81.00 -49.00   0.50   62.00    --  -92.00 -75.00-122.31   64
 29  ω   -125.00 -49.00   0.50   62.00    --  -92.00 -77.00  60.00  152
 30  ω    -55.00 -24.00   0.50   62.00    --  -92.00 111.00-150.00   62
 31  ω   -177.00-136.00   0.50   62.00    --  -92.00 -76.00-162.48   82
 32  ω    -89.00 -49.00   0.50   62.00    --  -92.00 -75.00  32.93   80
 33  ω   -175.00 -49.00   0.50   62.00    --  -92.00 -77.00 -22.17  252
 34  ω   -176.00-150.00   0.50   62.00    --  -92.00 -77.00 108.35   52
 35  ω    -87.00 -49.00   0.50   62.00    --  -92.00 -77.00 -13.05   76
 36  ω    -74.00 -49.00   0.50   62.00    --  -92.00 -77.00 108.35   50
 37  ω   -107.00 -49.00   0.50   62.00    --  -92.00 -76.00  19.30  116
 38  ω   -177.00-107.00   0.50   62.00    --  -92.00 -75.00-147.94  140
 39  ω    -85.00 -49.00   0.50   62.00    --  -92.00 -77.00  -3.87   72
 40  ω   -108.00 -59.00   0.50   62.00    --  -92.00 111.00-150.00   98
 41  ω   -137.00-111.00   0.50   62.00    --  -92.00 -75.00  32.93   52
 42  ω   -177.00-132.00   0.50   62.00    --  -92.00 -77.00  -3.87   90
 43  ω    -75.00 -49.00   0.50   62.00    --  -92.00 -75.00 -42.65   52
 44  ω    -79.00 -49.00   0.50   62.00    --  -92.00 -75.00 -74.94   60
 45  ω   -144.00-118.00   0.50   62.00    --  -92.00 -75.00 -74.94   52
 46  ω   -111.00 -49.00   0.50   62.00    --  -92.00 -77.00 150.00  124
 47  ω    -76.00 -49.00   0.50   62.00    --  -92.00 -77.00  71.05   54
 48  ω    -74.00 -49.00   0.50   62.00    --  -92.00 -76.00  94.53   50
 49  ω   -176.00-135.00   0.50   62.00    --  -92.00 -77.00-180.00   82
 50  ω   -161.00-134.00   0.50   62.00    --  -92.00 -77.00   4.34   54
 51  ω   -117.00 -49.00   0.50   62.00    --  -92.00 -77.00   4.34  136
 52  ω    -74.00 -49.00   0.50   62.00    --  -92.00 -77.00 168.17   50
 53  ω   -105.00 -33.00   0.50   62.00    --  -92.00 111.00   0.00  144
 54  ω    -90.00 -49.00   0.50   62.00    --  -92.00 -77.00 124.58   82
 55  ω   -173.00-148.00   0.50   62.00    --  -92.00 -76.00-130.59   50
 56  ω    -81.00 -49.00   0.50   62.00    --  -92.00 -76.00-130.59   64
 57  ω   -170.00-145.00   0.50   62.00    --  -92.00 -77.00 150.00   50
 58  ω    -76.00 -49.00   0.50   62.00    --  -92.00 -77.00 -90.00   54
 59  ω   -176.00-150.00   0.50   62.00    --  -92.00 -77.00 138.05   52
 60  ω   -112.00 -49.00   0.50   62.00    --  -92.00 -77.00 138.05  126
 61  ω   -119.00 -93.00   0.50   62.00    --  -92.00 -76.00  94.53   52
 62  ω   -128.00 -96.00   0.50   62.00    --  -92.00 -77.00 -13.05   64
 63  ω   -145.00 -91.00   0.50   62.00    --  -92.00 -75.00 -42.65  108
 64  ω   -127.00-101.00   0.50   62.00    --  -92.00 -77.00 108.35   52
 65  ω   -139.00-113.00   0.50   62.00    --  -92.00 -75.00  44.69   52
 66  ω    -79.00 -49.00   0.50   62.00    --  -92.00 -75.00  44.69   60
 67  ω   -146.00-107.00   0.50   62.00    --  -92.00 -77.00 168.17   78
 68  ω   -150.00-124.00   0.50   62.00    --  -92.00 -76.00-108.54   52
 69  ω   -100.00 -49.00   0.50   62.00    --  -92.00 -76.00-108.54  102
 70  ω   -117.00 -82.00   0.50   62.00    --  -92.00 -77.00 -90.00   70
 71  ω   -145.00-119.00   0.50   62.00    --  -92.00 -77.00  71.05   52
 72  ω    -76.00 -49.00   0.50   62.00    --  -92.00 -75.00-147.94   54
 73  ω   -168.00-142.00   0.50   62.00    --  -92.00 -76.00 -83.50   52
 74  ω    -91.00 -49.00   0.50   62.00    --  -92.00 -76.00 -83.50   84
 75  ω     82.00 133.00   0.50   62.00    --   99.01 111.00 -30.00  102
 76  ω    118.00 157.00   0.50   62.00    --   99.01  77.00-180.00   78
 77  ω     56.00 114.00   0.50   62.00    --   99.01  77.00-180.00  116
 78  ω     56.00 157.00   0.50   62.00    --   99.01  77.00  30.00  202
 79  ω     56.00 156.00   0.50   62.00    --   99.01  77.00  90.00  200
 80  ω      9.00  53.00   0.50   62.00    --   99.01 -94.00-180.00   88
 81  ω    109.00 134.00   0.50   62.00    --   99.01 -88.00-114.84   50
 82  ω     66.00 156.00   0.50   62.00    --   99.01  77.00-120.00  180
 83  ω      9.00 102.00   0.50   62.00    --   99.01 -88.00-114.84  186
 84  ω    122.00 147.00   0.50   62.00    --   99.01 -87.00  26.11   50
 85  ω     68.00 117.00   0.50   62.00    --   99.01 -87.00  26.11   98
 86  ω    106.00 146.00   0.50   62.00    --   99.01 -85.00 -67.92   80
 87  ω      9.00  21.50   0.50   62.00    --   99.01 -87.00  26.11   25
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at home/near, HyPix'
_diffrn_measurement_method       'ω scans'
_diffrn_orient_matrix_type       
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.0680994000
_diffrn_orient_matrix_UB_12      -0.0409611000
_diffrn_orient_matrix_UB_13      0.0496646000
_diffrn_orient_matrix_UB_21      -0.0036795000
_diffrn_orient_matrix_UB_22      0.0349905000
_diffrn_orient_matrix_UB_23      0.0828323000
_diffrn_orient_matrix_UB_31      -0.0733158000
_diffrn_orient_matrix_UB_32      -0.0397881000
_diffrn_orient_matrix_UB_33      0.0217033000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Mo) X-ray Source'
_reflns_Friedel_coverage         0.934
_reflns_Friedel_fraction_full    1.000
_reflns_Friedel_fraction_max     0.986
_reflns_number_gt                15709
_reflns_number_total             17621
_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;
_reflns_threshold_expression     'I > 2σ(I)'
_computing_cell_refinement       'CrysAlisPro 1.171.42.36a (Rigaku OD, 2021)'
_computing_data_collection       'CrysAlisPro 1.171.42.36a (Rigaku OD, 2021)'
_computing_data_reduction        'CrysAlisPro 1.171.42.36a (Rigaku OD, 2021)'
_computing_molecular_graphics    'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'olex2.solve 1.5 (Bourhis et al., 2015)'
_refine_diff_density_max         1.343
_refine_diff_density_min         -0.593
_refine_diff_density_rms         0.094
_refine_ls_abs_structure_details 
;
 Flack x determined using 6570 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   0.06(16)
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.040
_refine_ls_hydrogen_treatment    refall
_refine_ls_matrix_type           full
_refine_ls_number_parameters     218
_refine_ls_number_reflns         17621
_refine_ls_number_restraints     10
_refine_ls_R_factor_all          0.0506
_refine_ls_R_factor_gt           0.0444
_refine_ls_restrained_S_all      1.057
_refine_ls_shift/su_max          14.346
_refine_ls_shift/su_mean         0.113
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0715P)²] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1143
_refine_ls_wR_factor_ref         0.1179
_refine_special_details          ?
_olex2_refinement_description    
;
1. Restrained distances
 O10-H10A
 0.952 with sigma of 0.02
 O10-H10B
 0.952 with sigma of 0.02
 O11-H11A
 0.952 with sigma of 0.02
 O11-H11B
 0.952 with sigma of 0.02
 O7-H7
 0.952 with sigma of 0.02
 O6-H6
 0.952 with sigma of 0.02
 O8-H8
 0.952 with sigma of 0.02
 O9-H9
 0.952 with sigma of 0.02
 N2-H2D
 0.8 with sigma of 0.02
;
_atom_sites_solution_hydrogens   difmap
_atom_sites_solution_primary     iterative
_atom_sites_solution_secondary   ?
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
O1 O 0.06319(6) 0.44385(4) 0.68750(7) 0.01069(5) Uani 1 1 d . . . . .
O2 O 0.24306(6) 0.29958(5) 0.53000(7) 0.01166(6) Uani 1 1 d . . . . .
O3 O 0.31420(7) 0.44619(4) 0.95184(6) 0.01115(6) Uani 1 1 d . . . . .
O4 O 0.49498(7) 0.30342(5) 0.79399(6) 0.01195(6) Uani 1 1 d . . . . .
O5 O 0.37996(6) 0.49770(4) 0.64351(5) 0.00810(4) Uani 1 1 d . . . . .
O6 O 0.19981(7) 0.63914(4) 0.81436(6) 0.00954(5) Uani 1 1 d D . . . .
O7 O 0.56577(7) 0.35028(6) 0.49451(6) 0.01361(7) Uani 1 1 d D . . . .
O8 O -0.08560(7) 0.27897(5) 0.49693(7) 0.01227(6) Uani 1 1 d D . . . .
O9 O 0.49778(7) 0.29138(5) 1.12259(6) 0.01203(6) Uani 1 1 d D . . . .
O10 O 0.06317(19) 0.87621(9) 0.94202(19) 0.0341(2) Uani 1 1 d D . . . .
O11 O 0.14951(11) 0.11372(8) 0.85189(11) 0.02041(10) Uani 1 1 d D . . . .
B1 B 0.24174(8) 0.50941(5) 0.77181(8) 0.00764(6) Uani 1 1 d . . . . .
B2 B 0.42137(8) 0.36466(6) 0.61207(8) 0.00872(7) Uani 1 1 d . . . . .
B3 B 0.07436(8) 0.34303(6) 0.57214(8) 0.00837(6) Uani 1 1 d . . . . .
B4 B 0.43707(9) 0.34731(6) 0.95314(8) 0.00855(6) Uani 1 1 d . . . . .
N1 N 0.25347(7) 0.10041(5) 0.27331(8) 0.01174(6) Uani 1 1 d . . . . .
N2 N 0.27296(9) 0.59516(5) 1.26859(7) 0.01210(6) Uani 1 1 d D . . . .
H1A H 0.160(4) 0.043(3) 0.297(4) 0.029(6) Uiso 1 1 d . . . . .
H1B H 0.215(3) 0.124(2) 0.155(3) 0.014(4) Uiso 1 1 d . . . . .
H1C H 0.255(5) 0.163(3) 0.345(5) 0.041(8) Uiso 1 1 d . . . . .
H1D H 0.375(4) 0.062(3) 0.295(4) 0.032(7) Uiso 1 1 d . . . . .
H2A H 0.296(3) 0.537(3) 1.188(3) 0.017(5) Uiso 1 1 d . . . . .
H2B H 0.337(5) 0.650(3) 1.254(5) 0.038(8) Uiso 1 1 d . . . . .
H2C H 0.157(4) 0.611(3) 1.252(4) 0.025(6) Uiso 1 1 d . . . . .
H2D H 0.311(5) 0.573(3) 1.376(3) 0.038(8) Uiso 1 1 d D . . . .
H6 H 0.151(4) 0.684(3) 0.710(3) 0.028(6) Uiso 1 1 d D . . . .
H7 H 0.511(2) 0.3516(16) 0.4376(19) -0.001(2) Uiso 1 1 d D . . A 1
H8 H -0.182(3) 0.304(3) 0.524(4) 0.028(6) Uiso 1 1 d D . . . .
H9 H 0.570(8) 0.221(4) 1.113(9) 0.11(2) Uiso 1 1 d D . . . .
H10A H 0.086(3) 0.7876(19) 0.936(3) 0.018(5) Uiso 1 1 d D . . . .
H10B H 0.107(7) 0.923(5) 0.848(5) 0.096(19) Uiso 1 1 d D . . . .
H11A H 0.159(2) 0.0330(13) 0.848(2) -0.001(2) Uiso 1 1 d D . . . .
H11B H 0.094(6) 0.173(4) 0.950(5) 0.055(10) Uiso 1 1 d D . . . .



_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
O1 B1 1.5025(7) . ?
O1 B3 1.3659(7) . ?
O5 B1 1.4619(7) . ?
O5 B2 1.4647(8) . ?
O3 B1 1.4889(7) . ?
O3 B4 1.3673(7) . ?
O6 B1 1.4494(7) . ?
O6 H6 0.92(2) . ?
O4 B4 1.3647(7) . ?
O4 B2 1.4928(7) . ?
O2 B2 1.4944(8) . ?
O2 B3 1.3700(7) . ?
O7 B2 1.4436(7) . ?
O7 H7 0.523(13) . ?
B4 O9 1.3740(7) . ?
B2 H7 1.510(15) . ?
B3 O8 1.3724(7) . ?
N2 H2A 0.88(3) . ?
N2 H2B 0.76(4) . ?
N2 H2C 0.84(3) . ?
N2 H2D 0.82(2) . ?
O8 H8 0.79(2) . ?
N1 H1A 0.94(3) . ?
N1 H1B 0.90(2) . ?
N1 H1C 0.84(4) . ?
N1 H1D 0.95(3) . ?
O9 H9 0.91(3) . ?
O11 H11A 0.858(14) . ?
O11 H11B 1.07(2) . ?
O10 H10A 0.95(2) . ?
O10 H10B 0.94(3) . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
B3 O1 B1 119.06(4) . . ?
B1 O5 B2 110.66(4) . . ?
B4 O3 B1 119.34(4) . . ?
B1 O6 H6 112.5(19) . . ?
B4 O4 B2 119.12(5) . . ?
B3 O2 B2 119.11(4) . . ?
B2 O7 H7 87.0(16) . . ?
O5 B1 O1 108.59(4) . . ?
O5 B1 O3 109.80(4) . . ?
O3 B1 O1 108.20(5) . . ?
O6 B1 O1 109.48(5) . . ?
O6 B1 O5 113.43(4) . . ?
O6 B1 O3 107.21(4) . . ?
O3 B4 O9 116.97(5) . . ?
O4 B4 O3 122.15(5) . . ?
O4 B4 O9 120.86(5) . . ?
O5 B2 O4 109.48(4) . . ?
O5 B2 O2 108.94(4) . . ?
O5 B2 H7 109.9(7) . . ?
O4 B2 O2 108.59(5) . . ?
O4 B2 H7 124.1(6) . . ?
O2 B2 H7 94.1(6) . . ?
O7 B2 O5 111.90(5) . . ?
O7 B2 O4 106.61(5) . . ?
O7 B2 O2 111.23(5) . . ?
O7 B2 H7 20.3(5) . . ?
O1 B3 O2 122.26(5) . . ?
O1 B3 O8 120.49(5) . . ?
O2 B3 O8 117.23(5) . . ?
H2A N2 H2B 105(3) . . ?
H2A N2 H2C 108(2) . . ?
H2A N2 H2D 111(3) . . ?
H2B N2 H2C 116(3) . . ?
H2B N2 H2D 103(3) . . ?
H2C N2 H2D 112(3) . . ?
B3 O8 H8 117(2) . . ?
H1A N1 H1B 103(2) . . ?
H1A N1 H1C 110(3) . . ?
H1A N1 H1D 111(3) . . ?
H1B N1 H1C 110(3) . . ?
H1B N1 H1D 115(2) . . ?
H1C N1 H1D 108(3) . . ?
B4 O9 H9 113(4) . . ?
H11A O11 H11B 130(3) . . ?
H10A O10 H10B 114(4) . . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
B1 O1 B3 O2 -0.18(9) . . . . ?
B1 O1 B3 O8 178.23(5) . . . . ?
B1 O5 B2 O4 -58.62(6) . . . . ?
B1 O5 B2 O2 60.00(5) . . . . ?
B1 O5 B2 O7 -176.60(4) . . . . ?
B1 O3 B4 O4 -0.55(9) . . . . ?
B1 O3 B4 O9 -179.22(5) . . . . ?
B4 O3 B1 O1 90.27(6) . . . . ?
B4 O3 B1 O5 -28.10(7) . . . . ?
B4 O3 B1 O6 -151.73(5) . . . . ?
B4 O4 B2 O5 29.65(7) . . . . ?
B4 O4 B2 O2 -89.18(7) . . . . ?
B4 O4 B2 O7 150.88(6) . . . . ?
B2 O5 B1 O1 -60.23(5) . . . . ?
B2 O5 B1 O3 57.89(5) . . . . ?
B2 O5 B1 O6 177.81(4) . . . . ?
B2 O4 B4 O3 -0.32(9) . . . . ?
B2 O4 B4 O9 178.30(6) . . . . ?
B2 O2 B3 O1 -0.24(9) . . . . ?
B2 O2 B3 O8 -178.70(5) . . . . ?
B3 O1 B1 O5 29.93(7) . . . . ?
B3 O1 B1 O3 -89.20(6) . . . . ?
B3 O1 B1 O6 154.26(5) . . . . ?
B3 O2 B2 O5 -29.13(7) . . . . ?
B3 O2 B2 O4 90.04(6) . . . . ?
B3 O2 B2 O7 -152.94(6) . . . . ?

_olex2_submission_special_instructions 'No special instructions were received'
_oxdiff_diffrn_reflns_filtered   3777
_oxdiff_exptl_absorpt_empirical_details 
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
;
_oxdiff_exptl_absorpt_empirical_full_max 1.548
_oxdiff_exptl_absorpt_empirical_full_min 0.719

# start Validation Reply Form
_vrf_SHFSU01_Independent_Atom_Model 
;
PROBLEM: The absolute value of parameter shift to su ratio > 0.20
RESPONSE: Problem caused by the disordered solvent molecules.
;
_vrf_PLAT080_Independent_Atom_Model 
;
PROBLEM: Maximum Shift/Error ............................      14.35 Why ? 
RESPONSE: Problem caused by the disordered solvent molecules.
;
_vrf_PLAT203_Independent_Atom_Model 
;
PROBLEM: Negative Isotropic ADP for H7        ...........     -0.001 Report
RESPONSE: This problem was improved in multipole model refinement in which hydrogen ADPs where
taken from SHADE (Simple Hydrogen Anisotropic Displacement Estimator)
;
_vrf_PLAT417_Independent_Atom_Model 
;
PROBLEM: Short Inter D-H..H-D       H10B     ..H11A     .       1.22 Ang.  
RESPONSE: This particular problem is caused by the disordered molecules of water. 
Hydrogens H10 and H11 belongs to these disordered solvent molecules.
;
####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
#######################################################################

data_Multipole_Model_Refinement
_database_code_depnum_ccdc_archive 'CCDC 2181472'
loop_
_audit_author_name
_audit_author_address
'Roman Gajda'
;University of Warsaw
Poland
;
_audit_update_record             
;
2022-06-23 deposited with the CCDC.	2022-09-07 downloaded from the CCDC.
;

# xd_geo

_chemical_formula_moiety         'B4 H4 O9, 2(H4 N), 2(H2 O)'
_chemical_formula_sum            'B4 H16 N2 O11'
_chemical_formula_weight         263.39
_chemical_absolute_configuration ?
_chemical_melting_point          ?
_chemical_oxdiff_formula         B4O11N2H16
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
B B 0.0013 0.0007 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_shelx_space_group_comment       
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;
_space_group_crystal_system      monoclinic
_space_group_IT_number           4
_space_group_name_H-M_alt        'P 1 21 1'
_space_group_name_Hall           'P 2yb'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, y+1/2, -z'

_cell_length_a                   7.16499(7)
_cell_length_b                   10.59066(11)
_cell_length_c                   7.24742(6)
_cell_angle_alpha                90
_cell_angle_beta                 98.6290(9)
_cell_angle_gamma                90
_cell_volume                     543.723(9)
_cell_formula_units_Z            2
_cell_measurement_reflns_used    51795
_cell_measurement_temperature    90.1(6)
_cell_measurement_theta_max      65.9010
_cell_measurement_theta_min      3.4460
_shelx_estimated_absorpt_T_max   ?
_shelx_estimated_absorpt_T_min   ?
_exptl_absorpt_coefficient_mu    0.159
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.73842
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.42.36a (Rigaku Oxford Diffraction, 2021)
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.609
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       irregular
_exptl_crystal_F_000             276
_exptl_crystal_size_max          0.27
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.12
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0555
_diffrn_reflns_av_unetI/netI     0.0410
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.997
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       26
_diffrn_reflns_limit_k_min       -26
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            94540
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.992
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         62.671
_diffrn_reflns_theta_min         3.433
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      90.1(6)
_diffrn_detector                 'Hybrid Pixel Array Detector'
_diffrn_detector_area_resol_mean 10.0000
_diffrn_detector_type            HyPix
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at home/near, HyPix'
_diffrn_measurement_method       'ω scans'
_diffrn_orient_matrix_type       
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.0680994000
_diffrn_orient_matrix_UB_12      -0.0409611000
_diffrn_orient_matrix_UB_13      0.0496646000
_diffrn_orient_matrix_UB_21      -0.0036795000
_diffrn_orient_matrix_UB_22      0.0349905000
_diffrn_orient_matrix_UB_23      0.0828323000
_diffrn_orient_matrix_UB_31      -0.0733158000
_diffrn_orient_matrix_UB_32      -0.0397881000
_diffrn_orient_matrix_UB_33      0.0217033000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Mo) X-ray Source'
_reflns_Friedel_coverage         0.934
_reflns_Friedel_fraction_full    1.000
_reflns_Friedel_fraction_max     0.986
_reflns_number_gt                15709
_reflns_number_total             17621
_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;
_reflns_threshold_expression     'I > 2σ(I)'
_computing_cell_refinement       'CrysAlisPro 1.171.42.36a (Rigaku OD, 2021)'
_computing_data_collection       'CrysAlisPro 1.171.42.36a (Rigaku OD, 2021)'
_computing_data_reduction        'CrysAlisPro 1.171.42.36a (Rigaku OD, 2021)'
_computing_molecular_graphics    'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'olex2.solve 1.5 (Bourhis et al., 2015)'


loop_
_atom_site_label
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_occupancy
_atom_site_symmetry_multiplicity
_atom_site_U_iso_or_equiv
O(1) 0.06330(6) 0.4420(7) 0.68761(6) 1 2 0.011
O(2) 0.24334(6) 0.2977(7) 0.53017(6) 1 2 0.012
O(3) 0.31420(7) 0.4444(7) 0.95190(5) 1 2 0.012
O(4) 0.49508(7) 0.3016(7) 0.79423(5) 1 2 0.012
O(5) 0.37999(5) 0.4958(7) 0.64383(4) 1 2 0.008
O(6) 0.19998(6) 0.6373(7) 0.81445(5) 1 2 0.010
O(7) 0.56627(6) 0.3483(7) 0.49500(5) 1 2 0.014
O(8) -0.08514(6) 0.2770(7) 0.49699(6) 1 2 0.013
O(9) 0.49750(7) 0.2896(7) 1.12288(5) 1 2 0.013
O(10) 0.0622(2) 0.8737(7) 0.9417(2) 1 2 0.034
O(11) 0.14935(10) 0.1120(7) 0.85215(9) 1 2 0.021
N(1) 0.25347(6) 0.0985(7) 0.27322(6) 1 2 0.012
N(2) 0.27281(7) 0.5932(7) 1.26861(5) 1 2 0.013
B(1) 0.24179(6) 0.5076(7) 0.77186(5) 1 2 0.008
B(2) 0.42139(6) 0.3628(7) 0.61210(5) 1 2 0.009
B(3) 0.07439(6) 0.3411(7) 0.57222(5) 1 2 0.009
B(4) 0.43719(6) 0.3454(7) 0.95321(5) 1 2 0.009
H(1A) 0.163676 0.043324 0.294675 1 2 0.028
H(1B) 0.212022 0.123782 0.155627 1 2 0.015
H(1C) 0.258643 0.165244 0.350748 1 2 0.036
H(1D) 0.369673 0.064348 0.29531 1 2 0.031
H(2A) 0.295647 0.534392 1.185131 1 2 0.017
H(2B) 0.346025 0.660589 1.255136 1 2 0.037
H(2C) 0.148675 0.611264 1.250249 1 2 0.025
H(2D) 0.31373 0.570691 1.387569 1 2 0.035
H(6) 0.152381 0.686292 0.706114 1 2 0.023
H(7) 0.478412 0.347775 0.381122 1 2 0.025
H(8) -0.201604 0.30998 0.527262 1 2 0.026
H(9) 0.571029 0.216385 1.103184 1 2 0.027
H(10A) 0.08593 0.784549 0.938413 1 2 0.019
H(10B) 0.10628 0.92254 0.84613 1 2 0.098
H(11A) 0.1589 0.03296 0.84731 1 2 0.000
H(11B) 0.100307 0.165045 0.94105 1 2 0.055



##
#  Local CIF definition in XD - coordinates of dummy atoms
##

loop_
_atom_local_dummy_label
_atom_local_dummy_fract_x
_atom_local_dummy_fract_y
_atom_local_dummy_fract_z
DUM0 0 0 0



loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_1
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
O(1) B(1) 1.5023(6) 1_555 1_555 yes
O(1) B(3) 1.3666(6) 1_555 1_555 yes
O(2) B(2) 1.4926(6) 1_555 1_555 yes
O(2) B(3) 1.3711(6) 1_555 1_555 yes
O(3) B(1) 1.4887(5) 1_555 1_555 yes
O(3) B(4) 1.3684(6) 1_555 1_555 yes
O(4) B(2) 1.4938(6) 1_555 1_555 yes
O(4) B(4) 1.3633(5) 1_555 1_555 yes
O(5) B(1) 1.4604(5) 1_555 1_555 yes
O(5) B(2) 1.4650(6) 1_555 1_555 yes
O(6) B(1) 1.4494(6) 1_555 1_555 yes
O(6) H(6) 0.960(4) 1_555 1_555 yes
O(7) B(2) 1.4441(5) 1_555 1_555 yes
O(7) H(7) 0.9600(4) 1_555 1_555 yes
O(8) B(3) 1.3702(6) 1_555 1_555 yes
O(8) H(8) 0.960(3) 1_555 1_555 yes
O(9) B(4) 1.3745(5) 1_555 1_555 yes
O(9) H(9) 0.960(6) 1_555 1_555 yes
O(10) H(10A) 0.960(7) 1_555 1_555 yes
O(10) H(10B) 0.955(4) 1_555 1_555 yes
O(11) H(11A) 0.842(7) 1_555 1_555 yes
O(11) H(11B) 0.960(4) 1_555 1_555 yes
N(1) H(1A) 0.900(5) 1_555 1_555 yes
N(1) H(1B) 0.900(2) 1_555 1_555 yes
N(1) H(1C) 0.900(6) 1_555 1_555 yes
N(1) H(1D) 0.900(3) 1_555 1_555 yes
N(2) H(2A) 0.900(5) 1_555 1_555 yes
N(2) H(2B) 0.900(6) 1_555 1_555 yes
N(2) H(2C) 0.9000(16) 1_555 1_555 yes
N(2) H(2D) 0.900(2) 1_555 1_555 yes


loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_2
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
B(1) O(1) B(3) 119.10(4) 1_555 1_555 1_555 yes
B(2) O(2) B(3) 119.16(4) 1_555 1_555 1_555 yes
B(1) O(3) B(4) 119.32(3) 1_555 1_555 1_555 yes
B(2) O(4) B(4) 119.15(4) 1_555 1_555 1_555 yes
B(1) O(5) B(2) 110.76(3) 1_555 1_555 1_555 yes
B(1) O(6) H(6) 113.4(4) 1_555 1_555 1_555 yes
B(2) O(7) H(7) 93.98(6) 1_555 1_555 1_555 yes
B(3) O(8) H(8) 115.5(3) 1_555 1_555 1_555 yes
B(4) O(9) H(9) 108.69(9) 1_555 1_555 1_555 yes
H(10A) O(10) H(10B) 115.8(3) 1_555 1_555 1_555 yes
H(11A) O(11) H(11B) 130.6(4) 1_555 1_555 1_555 yes
H(1A) N(1) H(1B) 102.3(2) 1_555 1_555 1_555 yes
H(1A) N(1) H(1C) 111.45(10) 1_555 1_555 1_555 yes
H(1A) N(1) H(1D) 112.0(7) 1_555 1_555 1_555 yes
H(1B) N(1) H(1C) 109.6(7) 1_555 1_555 1_555 yes
H(1B) N(1) H(1D) 116.94(9) 1_555 1_555 1_555 yes
H(1C) N(1) H(1D) 104.7(2) 1_555 1_555 1_555 yes
H(2A) N(2) H(2B) 107.94(8) 1_555 1_555 1_555 yes
H(2A) N(2) H(2C) 108.9(3) 1_555 1_555 1_555 yes
H(2A) N(2) H(2D) 113.3(7) 1_555 1_555 1_555 yes
H(2B) N(2) H(2C) 113.2(7) 1_555 1_555 1_555 yes
H(2B) N(2) H(2D) 101.7(3) 1_555 1_555 1_555 yes
H(2C) N(2) H(2D) 111.76(6) 1_555 1_555 1_555 yes
O(1) B(1) O(3) 108.17(4) 1_555 1_555 1_555 yes
O(1) B(1) O(5) 108.61(3) 1_555 1_555 1_555 yes
O(1) B(1) O(6) 109.54(4) 1_555 1_555 1_555 yes
O(3) B(1) O(5) 109.76(3) 1_555 1_555 1_555 yes
O(3) B(1) O(6) 107.18(3) 1_555 1_555 1_555 yes
O(5) B(1) O(6) 113.45(3) 1_555 1_555 1_555 yes
O(2) B(2) O(4) 108.60(4) 1_555 1_555 1_555 yes
O(2) B(2) O(5) 108.99(4) 1_555 1_555 1_555 yes
O(2) B(2) O(7) 111.36(4) 1_555 1_555 1_555 yes
O(4) B(2) O(5) 109.35(3) 1_555 1_555 1_555 yes
O(4) B(2) O(7) 106.47(4) 1_555 1_555 1_555 yes
O(5) B(2) O(7) 111.98(4) 1_555 1_555 1_555 yes
O(1) B(3) O(2) 122.16(4) 1_555 1_555 1_555 yes
O(1) B(3) O(8) 120.61(4) 1_555 1_555 1_555 yes
O(2) B(3) O(8) 117.21(4) 1_555 1_555 1_555 yes
O(3) B(4) O(4) 122.16(4) 1_555 1_555 1_555 yes
O(3) B(4) O(9) 116.84(4) 1_555 1_555 1_555 yes
O(4) B(4) O(9) 120.98(4) 1_555 1_555 1_555 yes



loop_
_atom_rho_multipole_atom_label
_atom_rho_multipole_coeff_Pv
_atom_rho_multipole_coeff_P00
_atom_rho_multipole_coeff_P11
_atom_rho_multipole_coeff_P1-1
_atom_rho_multipole_coeff_P10
_atom_rho_multipole_coeff_P20
_atom_rho_multipole_coeff_P21
_atom_rho_multipole_coeff_P2-1
_atom_rho_multipole_coeff_P22
_atom_rho_multipole_coeff_P2-2
_atom_rho_multipole_coeff_P30
_atom_rho_multipole_coeff_P31
_atom_rho_multipole_coeff_P3-1
_atom_rho_multipole_coeff_P32
_atom_rho_multipole_coeff_P3-2
_atom_rho_multipole_coeff_P33
_atom_rho_multipole_coeff_P3-3
_atom_rho_multipole_coeff_P40
_atom_rho_multipole_coeff_P41
_atom_rho_multipole_coeff_P4-1
_atom_rho_multipole_coeff_P42
_atom_rho_multipole_coeff_P4-2
_atom_rho_multipole_coeff_P43
_atom_rho_multipole_coeff_P4-3
_atom_rho_multipole_coeff_P44
_atom_rho_multipole_coeff_P4-4
_atom_rho_multipole_kappa
_atom_rho_multipole_kappa_prime0
_atom_rho_multipole_kappa_prime1
_atom_rho_multipole_kappa_prime2
_atom_rho_multipole_kappa_prime3
_atom_rho_multipole_kappa_prime4
_atom_rho_multipole_radial_slater_n0
_atom_rho_multipole_radial_slater_zeta0
_atom_rho_multipole_radial_slater_n1
_atom_rho_multipole_radial_slater_zeta1
_atom_rho_multipole_radial_slater_n2
_atom_rho_multipole_radial_slater_zeta2
_atom_rho_multipole_radial_slater_n3
_atom_rho_multipole_radial_slater_zeta3
_atom_rho_multipole_radial_slater_n4
_atom_rho_multipole_radial_slater_zeta4
O(1) 7.02(5) 0 -0.013(16) -0.104(13) 0.035(18) 0.010(12) -0.016(12) -0.004(12)
-0.025(12) -0.003(13) 0.044(18) -0.014(19) -0.009(18) 0.081(18) -0.002(16)
0.044(17) 0.025(17) -0.01(2) -0.022(18) 0.009(17) -0.027(19) 0.010(19)
-0.022(18) 0.005(19) -0.027(18) -0.006(19) 0.9517(15) 1 1 1 1 1 2 4.466 2 4.466
2 4.466 3 4.466 4 4.466
O(2) 6.93(5) 0 -0.016(16) -0.135(17) 0.118(15) 0.043(13) -0.023(13) 0.011(11)
0.014(12) 0.005(12) 0.07(2) 0.014(18) -0.004(17) 0.043(19) 0.006(18) 0.013(19)
0.005(17) -0.00(2) 0.032(19) -0.016(18) -0.01(2) 0.01(2) -0.041(19) 0.019(19)
-0.003(18) 0.038(19) 0.9517(15) 1 1 1 1 1 2 4.466 2 4.466 2 4.466 3 4.466 4
4.466
O(3) 6.94(5) 0 0.067(16) 0.026(13) 0.063(18) -0.009(13) -0.028(13) 0.002(11)
-0.018(12) 0.023(12) 0.071(19) 0.05(2) -0.024(18) 0.059(18) 0.010(15)
-0.012(17) 0.009(17) 0.01(2) -0.00(2) 0.006(17) -0.01(2) -0.038(19) 0.052(19)
0.013(19) -0.005(18) 0.018(18) 0.9517(15) 1 1 1 1 1 2 4.466 2 4.466 2 4.466 3
4.466 4 4.466
O(4) 6.86(5) 0 -0.095(17) 0.077(17) -0.166(14) 0.016(12) 0.004(13) -0.035(11)
-0.015(13) 0.015(13) 0.067(19) -0.007(17) 0.028(16) 0.085(19) -0.029(18)
0.000(19) -0.006(18) 0.02(2) 0.014(19) 0.031(17) 0.008(19) 0.03(2) 0.042(19)
0.007(19) -0.007(19) -0.02(2) 0.9517(15) 1 1 1 1 1 2 4.466 2 4.466 2 4.466 3
4.466 4 4.466
O(5) 6.86(5) 0 0.140(11) 0.01(2) -0.069(12) -0.010(11) 0.007(10) -0.011(11)
0.029(10) -0.020(11) 0.065(14) -0.016(14) -0.031(19) 0.023(14) 0.00(2)
0.014(13) -0.02(2) 0.004(18) -0.024(16) 0.017(18) 0.006(17) 0.018(17)
-0.014(17) 0.011(18) -0.028(16) 0.016(16) 0.9517(15) 1 1 1 1 1 2 4.466 2 4.466
2 4.466 3 4.466 4 4.466
O(6) 6.89(5) 0 -0.088(13) 0.066(17) 0.072(15) -0.016(12) -0.042(11) 0.057(11)
0.022(11) -0.036(11) 0.07(2) -0.072(17) 0.090(14) 0.028(17) -0.015(17)
0.022(18) -0.050(17) 0.023(18) -0.056(17) 0.002(17) 0.010(17) -0.031(18)
0.039(18) 0.031(17) -0.028(17) -0.005(17) 0.9517(15) 1 1 1 1 1 2 4.466 2 4.466
2 4.466 3 4.466 4 4.466
O(7) 6.67(5) 0 -0.03(2) 0.033(12) 0.449(12) 0.405(12) -0.063(14) 0.100(11)
-0.091(13) -0.012(15) 0.294(16) -0.03(2) 0.015(14) 0.050(15) -0.03(2) -0.01(2)
-0.006(17) 0.12(2) -0.01(2) -0.008(16) 0.007(19) -0.01(2) -0.04(2) 0.04(2)
0.01(2) -0.02(2) 0.9517(15) 1 1 1 1 1 2 4.466 2 4.466 2 4.466 3 4.466 4 4.466
O(8) 6.77(5) 0 -0.034(16) -0.063(17) 0.260(15) 0.049(13) -0.015(12) 0.068(12)
-0.017(12) 0.044(12) 0.18(2) 0.046(18) 0.059(17) -0.012(19) -0.016(18)
-0.038(18) 0.036(17) 0.04(2) -0.019(19) 0.014(18) -0.017(19) -0.034(19)
0.022(19) 0.014(19) 0.025(18) -0.009(18) 0.9517(15) 1 1 1 1 1 2 4.466 2 4.466 2
4.466 3 4.466 4 4.466
O(9) 6.84(5) 0 -0.041(16) 0.106(13) 0.162(18) 0.004(13) -0.020(12) 0.031(12)
-0.036(12) -0.015(12) 0.071(18) -0.04(2) -0.015(18) -0.010(17) -0.014(16)
-0.015(16) 0.066(17) -0.06(2) -0.07(2) -0.061(18) -0.008(19) -0.018(19)
0.011(19) -0.051(19) 0.032(18) 0.001(18) 0.9517(15) 1 1 1 1 1 2 4.466 2 4.466 2
4.466 3 4.466 4 4.466
O(10) 6.37(6) 0 0.119(18) -0.19(2) 0.29(2) 0.22(2) 0.25(2) -0.026(17) -0.29(2)
0.01(2) 0.09(3) 0.18(3) -0.28(2) 0.00(3) -0.30(3) -0.02(3) 0.09(3) -0.10(4)
0.10(4) -0.02(3) 0.03(3) -0.17(3) -0.19(3) -0.08(3) 0.02(3) 0.02(3) 0.9517(15)
1 1 1 1 1 2 4.466 2 4.466 2 4.466 3 4.466 4 4.466
O(11) 4.98(6) 0 0.021(13) -0.036(15) -0.02(2) -0.146(17) 0.009(15) 0.021(15)
-0.126(14) 0.059(14) 0.03(3) -0.02(2) 0.07(2) 0.03(2) -0.00(2) -0.061(17)
0.050(18) 0.18(3) 0.01(2) -0.00(2) 0.00(2) 0.02(2) 0.04(2) -0.04(2) 0.09(2)
0.03(2) 0.9517(15) 1 1 1 1 1 2 4.466 2 4.466 2 4.466 3 4.466 4 4.466
N(1) 6.05(12) 0 0.059(17) -0.17(2) -0.02(2) -0.009(16) 0.035(15) -0.035(15)
-0.024(15) 0.006(15) 0.13(2) -0.10(2) -0.02(2) -0.07(2) -0.03(2) -0.13(2)
-0.13(2) 0.03(3) 0.03(2) -0.05(2) 0.00(2) 0.03(2) 0.06(2) 0.08(2) 0.02(2)
-0.06(2) 0.955(5) 1 1 1 1 1 2 3.83936 2 3.83936 2 3.83936 3 3.83936 4 3.83936
N(2) 6.07(11) 0 -0.091(19) 0.038(17) 0.03(2) -0.023(16) -0.026(15) -0.006(15)
0.023(15) -0.027(14) 0.15(2) 0.00(2) 0.02(2) -0.02(2) -0.045(19) -0.01(2)
-0.13(2) 0.06(3) 0.07(2) -0.06(2) 0.01(2) 0.02(2) 0.04(2) 0.04(2) -0.06(2)
0.02(2) 0.955(5) 1 1 1 1 1 2 3.83936 2 3.83936 2 3.83936 3 3.83936 4 3.83936
B(1) 2.69(9) 0 -0.03(3) -0.06(3) -0.18(4) 0.14(3) -0.08(3) 0.02(3) 0.05(3)
0.04(3) 0.25(4) -0.03(4) 0.05(4) 0.02(4) -0.07(4) -0.03(4) -0.15(4) -0.00(6)
0.11(5) 0.19(5) -0.04(5) -0.01(5) 0.07(5) 0.16(5) 0.11(5) 0.00(4) 1.096(10) 1 1
1 1 1 2 2.5246 2 2.5246 2 2.5246 3 2.5246 4 2.5246
B(2) 2.49(9) 0 0.18(3) -0.00(4) 0.13(3) 0.15(3) 0.11(3) 0.04(3) -0.08(3)
0.02(3) 0.28(4) 0.08(3) 0.11(5) 0.02(4) 0.11(4) 0.06(4) -0.16(4) 0.14(5)
0.02(5) -0.04(5) 0.04(5) 0.04(5) 0.04(5) 0.09(5) 0.03(5) 0.03(5) 1.096(10) 1 1
1 1 1 2 2.5246 2 2.5246 2 2.5246 3 2.5246 4 2.5246
B(3) 2.45(9) 0 -0.15(4) -0.19(3) -0.06(4) 0.13(3) -0.03(3) 0.07(3) -0.18(3)
0.02(3) 0.32(4) -0.12(4) -0.04(4) 0.24(4) -0.02(4) -0.03(4) -0.00(4) -0.15(6)
0.09(5) -0.07(5) -0.02(5) 0.06(5) -0.03(5) -0.17(5) 0.10(5) 0.04(5) 1.096(10) 1
1 1 1 1 2 2.5246 2 2.5246 2 2.5246 3 2.5246 4 2.5246
B(4) 2.27(9) 0 0.10(4) 0.04(4) 0.13(3) 0.11(3) 0.04(3) 0.05(3) -0.25(3) 0.07(3)
0.29(5) -0.01(4) 0.08(4) 0.14(4) 0.07(4) 0.04(4) -0.09(4) 0.15(6) -0.09(4)
-0.03(5) -0.11(5) 0.03(5) 0.02(5) -0.15(5) 0.11(5) -0.10(5) 1.096(10) 1 1 1 1 1
2 2.5246 2 2.5246 2 2.5246 3 2.5246 4 2.5246
H(1A) 0.52(4) 0 0 0 0.13(4) 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 1.28(2) 1
1 1 1 1 0 2 1 2 2 2 3 2 4 2
H(1B) 0.64(4) 0 0 0 0.09(4) 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 1.28(2) 1
1 1 1 1 0 2 1 2 2 2 3 2 4 2
H(1C) 0.50(4) 0 0 0 0.07(4) 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 1.28(2) 1
1 1 1 1 0 2 1 2 2 2 3 2 4 2
H(1D) 0.63(4) 0 0 0 -0.02(5) 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 1.28(2)
1 1 1 1 1 0 2 1 2 2 2 3 2 4 2
H(2A) 0.53(4) 0 0 0 0.06(4) 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 1.28(2) 1
1 1 1 1 0 2 1 2 2 2 3 2 4 2
H(2B) 0.56(4) 0 0 0 0.10(4) 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 1.28(2) 1
1 1 1 1 0 2 1 2 2 2 3 2 4 2
H(2C) 0.48(4) 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 1.28(2) 1 1 1 1
1 0 2 1 2 2 2 3 2 4 2
H(2D) 0.65(4) 0 0 0 -0.01(4) 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 1.28(2)
1 1 1 1 1 0 2 1 2 2 2 3 2 4 2
H(6) 0.64(4) 0 0 0 0.01(4) 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 1.28(2) 1
1 1 1 1 0 2 1 2 2 2 3 2 4 2
H(7) 0.18(3) 0 0 0 0.06(3) 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 1.28(2) 1
1 1 1 1 0 2 1 2 2 2 3 2 4 2
H(8) 0.47(3) 0 0 0 -0.06(4) 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 1.28(2) 1
1 1 1 1 0 2 1 2 2 2 3 2 4 2
H(9) 0.57(4) 0 0 0 0.21(4) 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 1.28(2) 1
1 1 1 1 0 2 1 2 2 2 3 2 4 2
H(10A) 0.58(4) 0 0 0 0.18(5) 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 1.28(2)
1 1 1 1 1 0 2 1 2 2 2 3 2 4 2
H(10B) 0.05(4) 0 0 0 -0.25(5) 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 1.28(2)
1 1 1 1 1 0 2 1 2 2 2 3 2 4 2
H(11A) 1.69(6) 0 0 0 0.43(5) 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 1.28(2)
1 1 1 1 1 0 2 1 2 2 2 3 2 4 2
H(11B) 0.17(3) 0 0 0 -0.23(4) 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 1.28(2)
1 1 1 1 1 0 2 1 2 2 2 3 2 4 2

##
# Local CIF definition in XD - local coordinate systems
##

loop_
_atom_local_axes_atom_label
_atom_local_axes_atom0
_atom_local_axes_ax1
_atom_local_axes_atom1
_atom_local_axes_atom2
_atom_local_axes_ax2
O(1) B(3) Z O(1) B(1) Y
O(2) B(3) Z O(2) B(2) Y
O(3) B(4) Z O(3) B(1) Y
O(4) B(4) Z O(4) B(2) Y
O(5) B(1) Z O(5) B(2) Y
O(6) H(6) Z O(6) B(1) Y
O(7) H(7) Z O(7) B(2) Y
O(8) H(8) Z O(8) B(3) Y
O(9) H(9) Z O(9) B(4) Y
O(10) H(10B) Z O(10) H(10A) Y
O(11) H(11A) Z O(11) H(11B) Y
N(1) H(1C) Z N(1) H(1B) Y
N(2) H(2B) Z N(2) H(2D) Y
B(1) O(6) Z B(1) O(5) Y
B(2) O(7) Z B(2) O(5) Y
B(3) O(1) Z B(3) O(2) Y
B(4) O(4) Z B(4) O(3) Y
H(1A) N(1) Z H(1A) H(1B) Y
H(1B) N(1) Z H(1B) H(1A) Y
H(1C) N(1) Z H(1C) H(1D) Y
H(1D) N(1) Z H(1D) H(1C) Y
H(2A) N(2) Z H(2A) H(2B) Y
H(2B) N(2) Z H(2B) H(2D) Y
H(2C) N(2) Z H(2C) H(2B) Y
H(2D) N(2) Z H(2D) H(2B) Y
H(6) O(6) Z H(6) B(1) Y
H(7) O(7) Z H(7) B(2) Y
H(8) O(8) Z H(8) B(3) Y
H(9) O(9) Z H(9) B(4) Y
H(10A) O(10) Z H(10A) H(10B) Y
H(10B) O(10) Z H(10B) H(10A) Y
H(11A) O(11) Z H(11A) H(11B) Y
H(11B) O(11) Z H(11B) H(11A) Y

##############################################################

# xd_lsm

# Refinement details

_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_number_restraints     0
_refine_ls_R_factor_gt           0.031
_refine_ls_R_factor_all          0.038
_refine_ls_R_Fsqd_factor         0.039
_refine_ls_wR_factor_ref         0.071
_refine_ls_hydrogen_treatment    ?
_refine_ls_number_reflns         13460
_refine_ls_number_parameters     460
_refine_ls_goodness_of_fit_ref   1.156
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
;
calc w2 = 1/[s²(Fo²)]
;
_refine_ls_shift/su_max          0.01514
_refine_ls_extinction_method     none
_refine_special_details          
;
?
;

##############################################################

# xd_fft

_refine_diff_density_max         0.571
_refine_diff_density_min         -0.308
_refine_diff_density_rms         0.058

# start Validation Reply Form

_vrf_PLAT417_Multipole_Model_Refinement 
;
PROBLEM: Short Inter D-H..H-D       H10B     ..H11A     .       1.26 Ang.  
RESPONSE: This particular problem is caused by the disordered molecules of water. 
Hydrogens H10 and H11 belongs to these disordered solvent molecules. 
;
# end Validation Reply Form
